硫堇瑞利共振散射荧光法测定肝素钠

目的：建立硫堇瑞利共振散射荧光法测定肝素钠的含量。方法：在近中性的Britton Robinson（B-R）缓冲溶液中，肝素钠与硫堇形成离子缔合物，在564 nm处生成新的瑞利共振散射（RRS）峰，随着肝素钠浓度的增加RRS峰显著增强。结果：在0.025~0.500 mg·L^-1范围内RRS强度与肝素钠浓度呈良好的线性关系，线性回归方程为ΔI=0.125+16.88C，平行6次测定，RSD为1.67%~3.01%，方法回收率为104.0%~106.4%。结论：硫堇染料作为增色剂的瑞利共振散射荧光法用于肝素钠注射液含量测定结果满意。

Objective: To establish a fluorescence and resonance Rayleigh scattering (RRS) with thionine to determine the content of heparin sodium. Methods: In the near-neutral Britton Robinson (BR) buffer solution,an ion-association complex was formed through the reaction of heparin sodium and thionine,a new RRS spectrum was found at 564 nm,and within a certain range,RRS intensity significantly increased with the increase of heparin sodium concentration. Results: The RRS intensity of the system was linear to the concentration of heparin sodium in the range of 0.025-0.500 mg·L^-1 and the linear regression equation was ΔI=0.125+16.88C.Meanwhile,the relative standard deviations were 1.67%-3.01% for six paralleled determinations,and recoveries were 104.0%-106.4%. Conclusion: The method developed in this paper is applied to the titer analysis of heparin sodium injection and satisfactory results are obtained.

1 ChP(中国药典)[S].1995.Vol Ⅱ(二部):307
2 LIU Shao-pu(刘绍璞), XU Hong(徐红), LUO Hong-qun(罗红群).Determination of heparin with basic triphenylmethane dyes by fading spectrophotometry(碱性三苯甲烷染料褪色分光光度法测定肝素钠)[J]. Chin J Anal Chem (分析化学), 2002, 30(6):712
3 Jiao QC, Liu Q, Sun C, et al.Investigation on the binging site in heparin by spectrophometry[J].Talanta, 1999, 48:1095
4 Jiao QC, Liu Q.Mechanism of interference and azur response in the heparin assay[J].Anal lett, 1998, 31(8):1311
5 SI Wen-hui(司文会), XIE Peng(解鹏).Spectrophotometric determination of heparin sodium salt by decoloration of night blue(夜蓝褪色分光光度法测定肝素钠)[J].Part B Chem Anal(理化检验-化学分册), 2010, 46(11):1334
6 MAO Ping(毛平), HUANG Xiao-lan(黄晓兰), LI Cui-zhen(李翠贞), et al. Determination of plasma heparin by high performance liquid chromatoagraphy(HPLC) and its clinical application(高效液相色谱法测定血浆肝素含量)[J].Chin J Med Lab Sci(中华医学检验杂志), 1995, 18(6):358
7 DING Kan(丁侃), FANG Ji-nian(方积年).Capillary electrophoresis of polysaccharides and its application(多糖类药物的毛细管电泳分析方法及其应用)[J].Chin J Chromatogr(色谱), 1999, 17(4):346
8 ZHANG Li(张莉), LI Na (李娜), ZHAO Feng - lin(赵凤林), et al. Research progress on glycosaminoglycans analysis(糖胺聚糖分析测定的研究进展)[J].Chin J Anal Chem(分析化学), 2005, 33(7):1023
9 Luo HQ, Liu SP, Liu ZF, et al.Resonance Rayleigh scattering spectra for studying the interaction of heparin with some basic phenothiazine dyes and their analytical applications[J].Anal Chim Acta, 2001, 449(1-2):261
10 Wei W, Wang H, Jiang CQ.Sepctrofluorimetric determination of trace heparin using lomefloxacin-terbium probe[J].Spectrochim Acta Part A, 2006, 63(2):241
11 Li J, Liu JK, Zhu XJ, et al.Spectrofluorimetric determination of heparin using doxycycline-europium probe[J].J Luminescence, 2005, 113(3-4):305
12 SHEN Di(沈迪), LING Zhu-san(凌柱三).Clinical Hemorrhage Pathology(临床出血病学)[M].Beijing(北京):People's Medical Publishing House(人民卫生出版社), 1996.84